ATOMIC FORCE MICROSCOPY

WORKING PRINCIPLE AND APPLICATIONS

Carlos Azucena

Introduction

AFM is a mechanical imaging instrument that measures the three dimensional topography as well as physical properties of a surface with a sharpened probe. Sharpened probe is positioned close enough to the surface such that can interact with the force fields associated with the surface

Probe

is very sharp, typically less than 50 nanometers in diameter and the areas scanned by the probe are less than 100 um.

Magnifications of the AFM may be between 100 X and 100,000,000 X.

AFMs at IFG

a)

b)
AFM Head Scanner Laser / Photodiode knobs

Objective/Condense r AFM Head

Scanner

Comparison to Other Microscopes

Because

of the sharper probe, greater resolution occur in AFM (App. 0.05NM)

Minimum sample preparation is required with an AFM

AFM is good for measuring mechanical properties of surfaces.

SEM / TEM
Samples Magnification Environment Time for image Horizontal Resolution Vertical Resolution Field of View Depth of Field Contrast on Flat Samples

AFM
Insulating / Conductive
3 Dimensional Vacuum / Air / Liquid 1 - 5 minute 0.2 nm .05 nm 100 um Poor Good

Must be conductive
2 Dimensional Vacuum 0.1 - 1 minute 0.2 nm (TEM) 5 nm (FE-SEM) n/a 100 nm (TEM) 1 mm (SEM) Good Poor

Operation Of AFM

Sample Preparation

Sample must be clean, If the surface is dirty with a thick contamination layer, it causes severe distortion in the image.

Sample must be rigidly mounted in stage If the sample is not mounted rigidly, it can vibrate. Vibrations reduced the resolution of the microscope and make it impossible to see small surface features.

Cantilever

Tip radius: 20nm

legs: 50um X 10um X, 0.5um

Platform. 10um X 5um, X 0.5um

Stiffness, 1 N/m
Resonant frequency, 200KHz

Thermal time constant, 1us

Tip height: 1.7um

AFM Modes of Operation

Topographic Mode Field Mode Material Sensing Mode Electrical Mode Lithographic Mode Mechanical Measurements Mode Thermal Measurements Mode

Topographic Mode

Three

basic regions of interaction between the probe and surface.

a) Free space b) Attractive region c) Repulsive region

Repulsive forces increase as the probe begins to "contact" the surface.

The repulsive forces in the AFM tend to cause the cantilever to bend up. Two primary methods for establishing the forces between a probe and a sample when an AFM is operated. a) Contact Mode b) Vibrating Mode

In contact mode the deflection of the cantilever is measured. A constant force is applied to the surface while scanning.

Contact mode is typically used for scanning hard samples and when a resolution of greater than 50 nanometers is required

Resonant frequencies of contact mode cantilevers are typically around 50 KHz and the force constants are below 1 N/m
In vibrating mode the changes in frequency and amplitude are used to measure the force interaction.

The setpoint is basically a measure of the force applied by the tip to the sample. In contact mode, it is a certain deflection of the cantilever. This deflection is maintained by the feedback electronics, so that the force between the tip and and sample is kept constant. In tapping mode, it is a certain amplitude (amplitude of oscillation of the cantilever), which controls the force with which the tip taps on the sample. Again, the set amplitude is maintained by the feedback electronics.

Vibrating methods are used when the highest resolution is required or if very soft samples are being scanned.

The probes used for vibrating mode are often less than 10 nm in diameter. The cantilevers have natural resonant frequency o given by

Contact Mode Images

Left: Bits on a compact disk. Center: Image of a metal surface. Right: Nano-particles on a surface.

Vibrating Mode Images Left: Silicon wafer. Center: Cancer cells. Right: Proteins

Set point

A large force applied to the sample, often means better imaging, but also means more wear on the tip, and the sample , i.e. lower tip life, and less chance of getting a complete sample without the tip getting contaminated / broken. So, generally you should start with a "safe" value of the setpoint (e.g. just touching the sample) and adjust it slowly until imaging does not improve anymore, then stop.

Phase imaging
Phase imaging refers to the monitoring of the phase lag between the signal that drives the cantilever oscillation and the cantilever oscillation output signal, Changes in the phase lag reflect changes in the mechanical properties of the sample surface. The systems feedback loop operates in the usual manner, using changes in the cantilevers deflection or vibration amplitude to measure sample topography. The phase lag is monitored while the topographic image is being taken so that images of topography and material properties can be collected simultaneously. One application of phase detection is to obtain material-properties information, especially for samples whose topography is best measured using True Non-Contact AFM rather than contact AFM (see True Non-Contact Mode).

Material Sensing Modes

In this mode we check the physical properties of materials. The amount of motion is in some way related to the differences in the chemical/physical properties of a surface Cantilever tends to twist while scanning

Twisting of the cantilever is measured in the light lever AFM by monitoring the left to right motion of the deflected laser light with a photo detector

Electrical Mode

Conductive AFM

probe may be used for measuring the electrical properties of a surface or structures located on the surface

Probe itself can be conductive or it can be made to be conductive by coating it with a metal layer

Electrical

properties are measured with a parametric tester tester is attached directly between the conductive AFM probe and the sample

Parametric

Mechanical Measuring Mode

Probe in an AFM may interact with the hard forces at a surface Such interaction allow making nano-mechanical measurements on a surface

Primary method for making mechanical measurement is the force/distance curve When the probe is pressed firmly into a surface, it may cause a nano-indentation of the surface

AFM Applications

Physical Sciences
Life Sciences High Technology

Software is available for automatically calculating the critical dimensions of DVD bits
DVD bits 11.7 x 11.7 u, B: CD R/W 23 x 23 u.

THANKS

Artifacts
Tip-sample convolution
This is an inherent feature of AFM and can never be fully removed. Any AFM image is a convolution of the shape of the probe, and the shape of the sample. This has the effect of making protruding features appear wide, and holes appear smaller (both narrower and often less deep, too). Broader (less sharp) probes will enhance the effect, as shown below.

Dirty or Contaminated Tips

If the tip is dirty or contaminated (often with parts of the sample sticking to it), you can get strange repeating shapes in the image. Sometimes it is obvious that this has occurred, but sometimes it is not. In the example below there are two images of the same sample, one taken with a clean tip, and one with a badly contaminated tip. Using a sample you already know can help you diagnose this problem

Blunt Tip
This artifact is common after scanning for a long time with the same tip. Tips may last very long, or sometimes go blunt quickly. Some samples (known as "tip-eaters") have a tendency to lead to blunt tips very quickly. In order to find out if your tip is blunt, scan a well-known sample like this one.

Artifacts
Double/multiple tips
if the tip is broken, or contaminated, you can often get a "double tip" effect, where both the tip and the contamination are scanning the surface. See the example below

Piezo Creep
Piezo creep occurs because when you apply a set voltage to the piezo(scanner), and then try to maintain it, in order to move to a certain location, the piezo tends to continue to move in the same direction for a certain period of time. Essentially, this means that when you start a new scan, you will get some stretching or compression of features at the beginnning of the image, and then the image will start to appear more normal over time. The effect will be particularly pronounced if you move to a new place within your scan range.

Edge Overshoot
This artifact occurs when the scanner moves further than it should vertically, leading to a very "sharp" edge on the features in the image. You can spot it in the topography profile as "bumps" on the edges of tall features. It's due to hysteresis in piezoelectric scanners.

Artifacts
Sample Drift
Sample drift means that your sample is moving as you try to scan it in the AFM. This artifact occurs in any type of SPM, or indeed any microscopy, but is much more serious in high resolution techniques like SEM, TEM and AFM than optical microscopy. It's known as "drift", because, in general, we see the sample moving slowly, in one direction (or expanding or contracting). You can generally recognize this as a "distortion" of the image, which changes when you change the slow scan direction. beginning of the image, and then the image will start to appear more normal over time. The effect will be particularly pronounced if you move to a new place within your scan range.
Laser Interference This effect is seen as broad "stripes" in your AFM images, running along the slow scan direction. They are caused by constructive interference between the reflection of the laser from the tip, and the reflection from the sample. Flying Tip This artifact shows that the AFM is not properly tracking the surface. In the example below the effect is obvious, but this is not always the case. Sometimes it is clearer if you look at some of the other signals, like amplitude or phase or deflection images. In the images shown below, note how all the features have a "tail" to their left.

Q/A
1. How does AFM work? 2. What's the difference between AFM and SPM? What are STM, SFM, etc? 3. What kind of samples can be analysed by AFM? What are the applications of AFM? 4. Can I see individual atoms with the AFM? 5. Can we scan in liquid? 6. Will it take long? (are we there yet?) 7. How big can my sample be? 8. How do I prepare my particulate sample (i.e. a powder)? 9. What concentration should I use to deposit dissolved or suspended particles? 10. Does my sample have to be clean? 11. What do I do with these strange files? 12. What if I want to do the analysis myself? 13. How do I use this software you recommended? 14. My image has weird horizontal lines all over it. 15. My image has weird vertical/diagonal bands lines all over it, or oscillations in the force curve. 16. What are Phase images? What are Amplitude images? 17. How do I use the AFM? 18. How can I see individual atoms with the AFM? 19. What is setpoint? Should I change it? 20. How do I optimise the feedback parameters? 21. What kind of artifacts can occur in AFM images? How can I avoid getting artifacts in my images? 22. I need to get an accurate height measurement. Should I calibrate?